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Zero order and signal processing spectrophotometric techniques applied for resolving interference of metronidazole with ciprofloxacin in their pharmaceutical dosage form
Abstract
Four rapid, simple, accurate and precise spectrophotometric methods were used for the determination of ciprofloxacin in the presence of metronidazole as interference. The methods under study are area under the curve, simultaneous equation in addition to smart signal processing techniques of manipulating ratio spectra namely Savitsky-Golay filters and continuous wavelet transform. All the methods were validated according to the ICH guidelines where accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can therefore be used for the routine analysis of ciprofloxacin in quality-control laboratories.
... Hence, the aim of the present work is to develop three accurate and precise spectrophotometric methods to determine aclidinium in the presence of formoterol as interferent compound in Duaklir ® Genuair ® and in their laboratory prepared mixtures. The methods under study are absorbance subtraction 18,19 , area under the curve 20 and simultaneous equation 20,21 . ...
... Hence, the aim of the present work is to develop three accurate and precise spectrophotometric methods to determine aclidinium in the presence of formoterol as interferent compound in Duaklir ® Genuair ® and in their laboratory prepared mixtures. The methods under study are absorbance subtraction 18,19 , area under the curve 20 and simultaneous equation 20,21 . ...
... The accuracy of the methods was determined by calculating the mean percent recovery of three determination of three different concentration of pure aclidinium bromide (20,30 and 40 μg /mL). The precision of the developed methods was checked by measuring percent relative standard deviation (% RSD) of three concentrations for aclidinium bromide (20, 30 and 40 μg /mL) repeated three times in the same day (repeatability) and in three days (intermediate precision). ...
Three simple, accurate and selective spectrophotometric methods were developed to determine aclidinium in the presence of formoterol as interferent compound in Duaklir ® Genuair ® inhalation powder. The methods under study are absorbance subtraction, area under the curve and simultaneous equation. The methods were linear over the concentration range of 5-50 μg/mL for aclidinium and validated according to the ICH guidelines. The accuracy and precision were found to be within the acceptable limits. The specificity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. Furthermore, the methods were statistically compared to the RP-HPLC method and good results were obtained.
... Several methods for analyzing CIP and MET in their mixture form or alone were discovered in the literature. CIP and MET were determined by spectrophotometric methods [7][8][9][10][11][12][13][14][15][16][17][18][19][20], reversed-phase ion-pair HPLC, TLCdensitometric methods [21], RP-UPLC Technique [22], LC methods [23,24], UPLC-mass [25], HPLC [26][27][28][29] and potentiometric & electrochemical determination [29][30][31][32]. ...
... The software PASW statistics 18 ® was used to do a oneway ANOVA statistical comparison of the suggested strategies. The computed F values were found to be lower than the expected values, indicating that there is no significant difference between the stated methodology and the recommended one [7] (Table 6). ...
Four simple, specific, easy, precise and accurate spectrophotometric methods were developed for the first time to examine ciprofloxacin and metronidazole in combination, without having been separated beforehand by the developed methods. Ciprofloxacin and metronidazole were determined by utilizing advanced absorbance subtraction (AAS), spectrum subtraction, bivariate and ratio difference methods. Precision, repeatability, robustness, and accuracy were all determined to be within acceptable levels after each of these procedures underwent validation in accordance with ICH recommendations. Each method’s benefits and drawbacks are illustrated, and the proposed and reported methodologies were statistically compared.
Supplementary Information
The online version contains supplementary material available at 10.1186/s13065-023-01007-z.
... Spectrophotometric methods [16][17][18][19], Potentiometric method [20] as well as chromatographic methods [20][21][22] were created and applied in mixed dosage forms to simultaneously quantify the binary combination of (CIP) and (MET). ...
... The absorption spectra of (CIP) and (MET) over the range of (200.0-380.0) nm were severely overlapped with each other when the pH control acidic solution was used as shown in Fig. 2. When compared with the spectra recorded in methanol and distilled water for the same sample of (CIP) and (MET) [18,19,55] the absorption band was slightly shifted in pH control acidic solution, as shown in Fig. 3, as a result the spectrophotometric methods for (CIP) and (MET) in methanol solvent as well as the distilled water could not be the best choice to determine the quantity of the cited drugs in dissolution tests due to the aliquots obtained from the vessels are completely different from the standards in methanol. Therefore, a different spectrophotometric approach is suggested in this paper to use the same (CIP) and (MET) standards, i.e. (CIP) and (MET) in pH control acidic solution, to quantify (CIP) and (MET) directly from the dissolution samples. ...
Objectives: The pharmaceutical industry and the National Regulatory Authorities (NRAs) are now focusing on the dissolution of multi-component drugs for quality control testing and predicting in vivo results to further consolidation of the biowaiver concept. The mixed formulation of Ciprofloxacin hydrochloride (CIP) and Metronidazole (MET) have been used as a model for simultaneous determination and obtaining in vitro dissolution profiles by using green analysis method namely (UV-CWT(Db4, a=490)).
Material and methods: The proposed method (UV-CWT(Db4, a=490)) includes UV detection combined with Continuous Wavelet Transform (CWT) with Daubechies family and the order of fourth at the scaling factor (a=490) has been used and validated for analyzing and obtaining the dissolution profiles of the fixed-dose combination (CIP-MET).
Results: The proposed method (UV-CWT(Db4, a=490)) has been validated effectively in accordance with ICH rules, regarding linearity, specificity, rigor, and preciseness of the working range (3.0–16.0 μg/mL) for both (CIP) and (MET), respectively. As well as figures of merit were concluded. The dissolution profiles of CIP-MET tablets were acquired by the proposed (UV-CWT (Db4, a=490)) and HPLC reported methods were conveniently compared using the indicators f1 and f2 ("difference" and "similarity") the results ensured that there were no statistically differences between the methods. In addition, the green assessment tool, namely analytical eco-scale, evaluated and compared the greenness of the suggested method (UV-CWT(Db4, a=490)) and HPLC reported one.
Conclusion: the suggested process (UV-CWT(Db4, a=490)) was considered as an excellent green, rapid, accurate, economical and minimum-steps method for simultaneously resolve and construct the dissolution curves of a fixed-dose combination drug (CIP-MET) in a short time and without the use of organic solvents, enabling significant labor and resource savings.
... Asides, selection of suitable stationary and mobile phases that give maximum peak capacity and selectivity are two critical parameters that needed to be carefully tuned [17]. On the other hand, spectrophotometric techniques provide a powerful alternative that can tackle the previous drawbacks with enhanced simplicity and usefulness for quality assurance testing of drug analysis [18,19]. However, severe spectral overlapping might be Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy 238 (2020) 118415 encountered when multiple analytes are simultaneously quantified [20,21]. ...
... Other parameters as the number of subsets, maximum number of LVs, and number of iterations at constant values were also estimated. It was found that GA reduced the number of variables in the absorbance matrix to about 19-28% of the original matrix (25,34,23,19, and 31 variables for ASP, SMT, ATN, RAM, and HCTZ respectively) resulting in simpler inputs. Asides, it also reduced latent variables of PLS models for ASP and RAM from seven to six leading to less complex models while it kept the same latent variables of SMT, ATN, and HCTZ as in the full PLS model (Fig. 3) but with improvement in their recoveries (Table 2). ...
Herein, UV spectrophotometry assisted by multivariate chemometric analysis has been presented for quantitative determination of complex quinary therapy containing atenolol, ramipril, hydrochlorothiazide, simvastatin and aspirin without any prior separation. Such combination is very useful for treating various cardiovascular diseases (CVD) including high blood pressure, hypercholesterolemia in addition to its antiplatelet aggregating activity. Calibration (15 samples) and validation (10 samples) sets were prepared of different concentrations for these drugs via implementing partial factorial experimental design. The zero order UV spectra of these sets were recorded and then subjected for further chemometric analysis. Partial least square (PLS) with/without variable selection procedure i.e. genetic algorithm (GA) were employed to untangle the UV spectral overlapping of these mixtures. The performance of these chemometric techniques are compared in terms of accuracy and predictive abilities using cross-validation and external validation methods. It was found that PLS provides good recoveries with prompt predictive ability albeit GA-PLS exhibits better analytical performance owing to its capability to remove redundant variables i.e. the number of absorbance variables has been reduced to about 19–28%. The developed methods have allowed for reliable determination of such complex therapy in its laboratory prepared mixtures and pharmaceutical preparation within comparable results to those reported by HPLC method, posing these chemometric methods as valuable and indispensable analytical tools in in-process testing and quality control analysis of many pharmaceutical compounds targeting CVD.
... In this paper, four different two-wavelength spectrophotometric methods were applied for cefoxitin sodium and its alkaline degradation productin binary mixture shaving overlapping spectra and for the removal of interference; namely: Dual wavelength (DW) [19][20][21] , Bivariate calibration spectrophotometric 19,22 , Simultaneous equation [23][24][25] , and Area under the curve (AUC) method 19,20,23 . ...
... In this paper, four different two-wavelength spectrophotometric methods were applied for cefoxitin sodium and its alkaline degradation productin binary mixture shaving overlapping spectra and for the removal of interference; namely: Dual wavelength (DW) [19][20][21] , Bivariate calibration spectrophotometric 19,22 , Simultaneous equation [23][24][25] , and Area under the curve (AUC) method 19,20,23 . ...
Four accurate and precise spectrophotometric methods were developedas stability-indicating methods for the determination of cefoxitin sodium in the presence of its alkaline degradation product. The proposed methods adopted for selective determination of intact cefoxitin sodium in the presence of up to 66.67% of its alkaline degradation product for dual wavelength, bivariate, and area under the curve methods and up to 83.33% for the simultaneous equation method. The methods obey Beers’s law in the range (4-36 μg ml-1) and were successfully applied for the determination of cefoxitin sodium in pure form and in pharmaceutical preparation. The results obtained were statistically analyzed and compared with those of a reported method, there are no significant differences between the proposed methods and the reported one.
... The literature survey revealed that several analytical techniques have been developed for the quantification of ciprofloxacin, lomefloxacin, and enrofloxacin alone or in combination with other medications or degradation products. These methods include UV spectrophotometry [7][8][9], spectrofluorimetry [9][10][11][12][13][14][15], electro-analytical techniques [16][17][18][19][20][21], and chromatographic methods such as HPLC [22][23][24][25] and LC-MS/MS [26][27][28][29]. Regarding their simultaneous determination, only chromatographic methods such as HPLC coupled with fluorescence detection [30] and micellar electrokinetic capillary chromatography [31] have been reported thus far, although these techniques may not be readily available in many quality control laboratories due to their high cost and complexity. ...
Herein, a novel UV spectrophotometric method coupled with chemometric tools was developed for the simultaneous determination of three fluoroquinolone antibiotics: ciprofloxacin, lomefloxacin, and enrofloxacin. Such integration of UV spectroscopy and chemometric analysis proved to be a simple, rapid, and cost-effective approach for the quantification of these clinically important pharmaceutical compounds and aid in their quality control analysis. The method employed firefly algorithm for variable selection and partial least squares (PLS) regression for model calibration. The developed method was validated by independent test set in addition the accuracy, intra and inter-day precision as per ICH guidelines which showed a satisfactory performance with mean recovery ranged between 98.18 and 101.83 with %RSD < 2. Besides, the developed method displayed ultrasensitive levels with LODs (0.0803, 0.1125, 0.1309 µg/mL) and LOQs (0.2434, 0.3409, 0.3968 µg/mL) for ciprofloxacin, lomefloxacin, and enrofloxacin, respectively. The greenness and blueness of the developed method were also evaluated using the recently proposed Analytical GREEnness metric approach (AGREE) and Blue applicability grade index (BAGI) tools, which showed a high AGREE score of 0.79 and a BAGI score of 77.5. These results indicate that the developed method provides an environmentally friendly alternative to the traditionally used chromatographic techniques, while maintaining high analytical practicability. Finally, the application of the developed methodology was demonstrated on real pharmaceutical and tap water samples, and the results were in good agreement with those obtained by the reference HPLC method indicating the reliability and suitability of the proposed spectrophotometric method for routine analysis of fluoroquinolone antibiotics.
... Furthermore, by merging mathematical manipulation processing stages with spectroscopic analysis, spectrum overlapping concerns may be addressed. The majority of these procedures rely on mathematical formulae or signal processing of the spectra, with no need for chemical or physicochemical separation [12][13][14][15]. However, very little literature has reported the application of such methods in DTG and LMV quantitative analysis [16][17][18]. ...
HIV treatment has greatly improved over the years, with the introduction of antiretroviral drugs that target the virus and suppress its replication. Dolutegravir and lamivudine are two such antiretroviral drugs that are commonly used in HIV treatment regimens. Herein, three spectrophotometric methods manipulating ratio spectra were developed for the simultaneous analysis of dolutegravir and lamivudine in their binary mixtures. These methods include mathematical processing stages like ratio difference method or signal processing approaches such as the first derivative of the ratio spectra, and continuous wavelet transform. The developed spectrophotometric methods exploit the characteristic spectral differences between dolutegravir and lamivudine in order to quantify them simultaneously. These methods have shown promising results in terms of sensitivity and selectivity as validated per the ICH guidelines. Moreover, these methods offer a straightforward and economical alternative to more intricate analytical methodologies like high-performance liquid chromatography. By incorporating the analytical eco-scale and AGREE for greenness evaluation of the proposed methods, we can further ensure that these techniques are effective and environmentally friendly, aligning with the principles of green chemistry. This evaluation will provide a comprehensive understanding of the environmental friendliness of these spectrophotometric methods in pharmaceutical analysis.
... Several methods for analyzing Ciprofloxacin and Metronidazole in their mixture form or alone were discovered in the literature. Ciprofloxacin and MET were determined by spectrophotometric methods, [58][59][60][61][62][63][64][65][66][67][68][69][70][71] Reversed-phase ion-pair HPLC, TLC-densitometric methods, 72 ...
Quality and safety of drugs are essential for effective therapeutic performance. Impurities can compromise the quality and safety of drugs, and they can arise during various stages of the development, production, storage and even transportation process. Therefore, detecting and measuring the number of impurities with high accuracy in drugs is necessary to ensure the quality and safety of drugs and to reduce the risks associated with taking them. Detecting and measuring impurities in drugs require advanced analytical techniques. The review highpoints a variety of analytical chemistry techniques include spectrophotometric and chromatographic methods in addition to some electrochemistry methods that have been applied for determination of certain drugs such as Ciprofloxacin, Metronidazole, Hydroxychloroquine and Cefotaxime in their pure form, combined form with other drugs, combined form with degradation products, and in biological fluids.
... Besides all of this, the time needed for optimization, the expensive tools required, and the hazardous organic reagents utilized are considered potential obstacles to that technique 31 . On the other hand, spectrophotometric techniques can overcome these previously mentioned drawbacks as it is fast, cheap, simple and time saving 32 . To this end, our aim is to simultaneously analyze NZ, PN, and three official impurities, namely; NZ impurity B, PN impurity A and PN impurity B, using simple chemometrics-assisted spectrophotometric methods. ...
This work is concerned with exploiting the power of chemometrics in the assay and purity determination of naphazoline HCl (NZ) and pheniramine maleate (PN) in their combined eye drops. Partial least squares (PLS) and artificial neural network (ANN) were the chosen models for that purpose where three selected official impurities, namely; NZ impurity B and PN impurities A and B, were successfully determined. The quantitative determinations of studied components were assessed by percentage recoveries, standard errors of prediction as well as root mean square errors of prediction. The developed models were constructed in the ranges of 5.0–13.0 μg mL⁻¹ for NZ, 10.0–60.0 μg mL⁻¹ for PN, 1.0–5.0 μg mL⁻¹ for NZ impurity B and 2.0–14.0 μg mL⁻¹ for two PN impurities. The proposed models could determine NZ and PN with respective detection limits of 0.447 and 1.750 μg mL⁻¹ for PLS, and 0.494 and 2.093 μg mL⁻¹ for ANN. The two established models were compared favorably with official methods where no significant difference observed.
... A combination of CP and MT was found to be effective for the management of mixed aerobic and anaerobic bacterial infections and Crohn's disease [3]. The review of literature highlighted some methods regarding the concurrent analysis of CP and MT in combination, including spectrophotometry [4][5][6] and HPLC techniques [7][8][9]. ...
... UV spectroscopy is a versatile technique that has been employed extensively for quantifications and analysis of many pharmaceutical compounds (14)(15)(16)(17). This technique has its own advantages over separation-based methods, including simplicity and a short analysis time (18). ...
Background
A recent combination of aspirin (ASP) and omeprazole (OMP) has been presented in a fixed dosage form for treatment of many CVD, particularly in patients with gastric diseases. However, ASP is very sensitive to degradation into salicylic acid (SAL) as its main degradation product. Hence, it is very important to develop methods for the determination of ASP and OMP in the presence of SAL.
Objective
In this study, UV spectrophotometry assisted by different univariate/multivariate post processing algorithms have been presented for quantitative determination of ASP, OMP and SAL without any prior separation.
Methods
The univariate/multivariate algorithms include double divisor ratio difference and double divisor mean centering as the univariate approaches while the multivariate methods include principal component regression (PCR) and partial least squares (PLS) models. Validation of the univariate methods was done according to the ICH guidelines while the multivariate models were validated using external validation set.
Results
The univariate algorithms displayed excellent regression and validation capabilities in terms of linearity, accuracy, precision, and selectivity. Regarding PCR and PLS, the number of latent variables were carefully optimized, and the model’s validation criteria displayed excellent recoveries and lower errors of prediction.
Conclusion
Our findings indicate that the developed methods were comparable to the only reported chromatographic methods but with much shorter analysis time and simplicity.
Highlights
Overall, this report presents the first spectrophotometric methods applied for determination of possible combination of ASP, OMP, and SAL, and poses theses methods as valuable analytical tools in in-process testing and quality control analysis.
... Unfortunately, These methods simultaneously deal with several variables, requiring the use of advanced statistical models as experimental design approaches, such as response surface methodology (RSM), consuming much time and effort [28][29][30]. These drawbacks were resolved by UV spectrophotometric strategies that can determine sophisticated mixtures [31][32][33][34][35][36]. ...
Cardiovascular disorders are among the foremost causes of death worldwide, especially hypertension, a silent killer syndrome that requires multiple drug therapy for proper monitoring. This work presents novel and green spectrophotometric methods for the concurrent analysis of Amlodipine (AML), Telmisartan (TEL), Hydrochlorothiazide (HCTZ), and Chlorthalidone (CLO) in their pharmaceutical dosage form. The suggested methods were Fourier-self deconvolution, amplitude factor, and first derivative methods developed and validated for the simultaneous determination of a tertiary mixture of AML, TEL, and HCTZ in TELVAS 3D 80 mg tablet and a binary mixture of TEL and CLO in TELMIKIND-CT 40 tablets. The investigated methods revealed limits of detection 0.7283 µg/ml for AML and ranging from 0.0121 to 0.0433, 0.15474 to 0.1767 µg/ml and 0.0578 to 0.1262 µg/ml for TEL, HCTZ, and CLO, respectively .The greenness of the suggested techniques was examined by an eco-scale scoring method called the penalty points, which revealed that the methods were excellent green regarding several parameters as reagents, instrument, and waste safety. The introduced methods’ validity was investigated by resolving prepared laboratory mixtures containing different AML, TEL, HCTZ, or TEL and CLO ratios. Furthermore, the introduced methods were ensured by the standard addition technique. Finally, the obtained results were statistically compared by the reported spectrophotometric methods, showing no significant difference concerning precision and accuracy.
... However, these methods require investigation of several variables at the same time using experimental design module, such as response surface methodology (RSM), that consume much time and effort due to the increased number of the required experiments [35]. The drawbacks of the electrochemical methods were overcome by UV spectrophotometric methods that have the ability to resolve sophisticated mixures [36][37][38][39][40][41]. Although the analysis of such complex mixtures by UV spectrophotometry requires some post mathematical processing mainly via chemometric analysis [42][43][44], however, the proposed UV spectrophotometric methods in this work had the ability to resolve the investigated drugs in mixtures without sophistication of the chemometric approaches. ...
Two newly introduced pharmaceutical mixtures of amlodipine/celecoxib and amlodipine/ramipril were developed to manage hypertension and the associated osteoarthritis. the current work presents three newly developed UV spectrophotometric methods depending on minimal mathematical manipulations on the zero-order spectrum namely: absorption correction, induced dual-wavelength, and Fourier self deconvoluted method; for the simultaneous determination of celecoxib and ramipril in their pharmaceutical combined dosage forms with amlodipine. In absorption correction and induced dual-wavelength method, celecoxib and ramipril were determined at 253 and 222 nm for absorption correction and (251-270 nm) and (222-230 nm) for induced dual-wavelength method, respectively from the zero-order spectrum after calculating the absorption correction and equality factors for amlodipine. Amlodipine itself was determined at 361 nm from the zero-order spectrum in both methods. In Fourier self deconvoluted method, celecoxib and amlodipine zero-order spectra were deconvoluted, using the spectrophotometer software built-in Fourier wavelet function, and then was determined at 360 and 269 nm, respectively. The proposed methods were simple, accurate, and sensitive requiring minimal mathematical manipulations saving the time needed for analysis. The methods were linear over the range of (5-60 μg/ml), (5-30 μg/ml), and (5-110 μg/ml) for each of amlodipine, celecoxib, and ramipril, respectively. The limit of detection was in the range of (0.5781 - 0.7132 μg/ml) for amlodipine, (0.6497 - 1.0450 μg/ml) for celecoxib, and (0.0001 - 0.0003 μg/ml) for ramipril that indicated the sensitivity of these suggested methods. All methods were validated as per ICH recommendations regarding linearity, range, accuracy, precision, and selectivity. A statistical comparative study executed for the proposed methods with each other and with the reported methods showed no significant difference between the proposed methods and the reported methods.
... In the present work, a comparative study using one-way ANOVA test was done between four methods as first reported spectrophotometric methods for the simultaneous determination of formoterol and fluticasone; namely simultaneous equation, [8][9][10][11] graphical absorbance ratio, 12-14 absorbance subtraction 15,16 and amplitude modulation. 17,18 Experiment Instruments SHIMADZU dual beam UV-visible spectrophotometer (Kyoto/ Japan), model UV-1650PC connected to IBM compatible and a HP1020 LaserJet printer. ...
... They have the advantages of simplicity and minimum time required for conducting the experiment. They are mainly divided into univariate [32][33][34] , bivariate 35 and multivariate analysis [36][37][38] . Each technique has its advantages and disadvantages. ...
The present work represents a simple, accurate, selective and sensitive UV-spectro-photometric methods for simultaneous estimation of xipamide and triamterene in pure and combined dosage form. The proposed methods are based on presence of iso-absorptive point. These methods include absorbance subtraction, amplitude modulation, Q analysis and absorbance ratio method. The methods have been validated for linearity, accuracy and precision and found to be rapid, precise and economical.
... The literature survey revealed that only three liquid chromatographic methods were used for estimation of simeprevir in plasma samples using tandem mass detection[4,5]and UV detection[6]. In this paper, five spectrophotometric methods were applied for the determination of simeprevir in the presence of its oxidative degradation product, namely; ratio difference[7,8], mean centering[7][8][9][10]and derivative ratio using Savitsky-Golay filters (SGF)[11][12][13], second derivative[14]and continuous wavelet transform (CWT)[15,16]. ...
Five simple spectrophotometric methods were developed for the determination of simeprevir in the presence of its oxidative degradation product namely, ratio difference, mean centering, derivative ratio using the Savitsky-Golay filters, second derivative and continuous wavelet transform. These methods are linear in the range of 2.5–40 μg/mL and validated according to the ICH guidelines. The obtained results of accuracy, repeatability and precision were found to be within the acceptable limits. The specificity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. Furthermore, these methods were statistically comparable to RP-HPLC method and good results were obtained. So, they can be used for the routine analysis of simeprevir in quality-control laboratories.
... It also has immense spectrum activity on both Gram-positive and Gram-negative bacteria and many microorganisms. [16,17] Several methods, including spectrophotometry, spectrofl uorometry, high-performance liquid chromatography (HPLC) with fl uorescence detection, HPLC with ultraviolet (UV) detection, liquid chromatography/ mass spectroscopy, capillary electrophoresis, and capillary electrophoresis, have been reported for ciprofl oxacin estimation in pharmaceutical and biological samples. Four rapid, simple, accurate, and precise spectrophotometric methods were used for the ciprofl oxacin determination in the presence of its acidic degradation product. ...
Background
The most important risk that threatens the skin wounds is infections. Therefore, fabrication of a membrane as a wound dressing with the ability of antibiotic delivery in a proper delivery rate is especially important.
Materials and Methods
Poly(glycerol sebacate) (PGS) was prepared from sebacic acid and glycerol with 1:1 ratio; then, it was added to gelatin in the 1:3 ratio and was dissolved in 80% (v/v) acetic acid, and finally, ciprofloxacin was added in 10% (w/v) of polymer solution. The gelatin/PGS membrane was fabricated using an electrospinning method. The membrane was cross-linked using ethyl-3-(3-dimethylaminopropyl) carbodiimide ethyl-3-(3-dimethylaminopropyl)carbodiim (EDC) and N-hydroxysuccinimide (NHS) in different time periods to achieve a proper drug release rate. Fourier-transform infrared (FTIR) spectroscopy was being used to manifest the peaks of polymers and drug in the membrane. Scanning electron microscopy (SEM) was used to evaluate the morphology, fibers diameter, pore size, and porosity before and after crosslinking process. Ultraviolet (UV)-visible spectrophotometry was used to show the ciprofloxacin release from the cross-linked membrane.
Results
FTIR analysis showed the characteristic peaks of gelatin, PGS, and ciprofloxacin without any added peaks after the crosslinking process. SEM images revealed that nanofibers’ size increased during the crosslinking process and porosity was higher than 80% before and after crosslinking process. UV-visible spectrophotometry showed the proper rate of ciprofloxacin release occurred from cross-linked membrane that remaining in EDC/NHS ethanol solution for 120 min.
Conclusion
The obtained results suggest that this recently developed gelatin/PGS membrane with controlled release of ciprofloxacin could be a promising biodegradable membrane for wound dressing.
... Therefore, it is necessary to develop a credible method for metronidazole determination with a high degree of selectivity and sensitivity. Several techniques have been employed for the detection and quantification of this drug, including the electrochemical sensor [26][27][28], Spectrophotometric [29,30], surface-enhanced Raman spectroscopy (SERS) [31], gas chromatography [32], high-performance liquid chromatography [33][34][35][36], and fluorescence spectrophotometry [28]. Nevertheless, most of these methods are deficient in simplicity, cost-effectiveness, and easy access. ...
In this research, g-C3N4nanosheets were facilely fabricated by thermal polymerization and then exfoliated into ultrathin nanosheets through ultrasonication in water media. Low-cost C-N nanosheets prepared by melamine possessed a highly π-conjugated structure and fluorescence property. In the present study, the g-C3N4nanosheet was used as a switch-off fluorescence sensor for rapid and sensitive sensing of metronidazole in biological fluids. These nanosheets were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. The fluorescence of the solution of the g-C3N4nanosheets was quenched effectively by metronidazole through two mechanisms: fluorescence resonance energy transfer and the formation of a donor−acceptor charge-transfer complex between π-electron rich donors. Under optimal conditions, the detection linear range for metronidazole was found to be from 0.01 to 0.10 μg ml⁻¹, with a limit of detection (LOD) of 0.008 μg ml⁻¹ which can cover standard range of metronidazole in real samples. Moreover, the proposed method has offered a green, rapid, and sensitive probe for quantitative determination of metronidazole in drug and biological fluids.
... They have been applied for resolving any overlapping spectra of two or more components present in the same mixture or formulation without any need for chemical or physicochemical separation. Some of these methods require data processing either application of mathematical equations for the overlapped zero order absorption spectra, derivatization of the zero spectra of the components or deriving and manipulation of the ratio spectra which may be followed by extra derivatization step [4][5][6]. ...
The first three UV spectrophotometric methods have been developed of simultaneous determination of two new FDA approved drugs namely; elbasvir and grazoprevir in their combined pharmaceutical dosage form. These methods include simultaneous equation, partial least squares with and without variable selection procedure (genetic algorithm). For simultaneous equation method, the absorbance values at 369 (λmax of elbasvir) and 253nm (λmax of grazoprevir) have been selected for the formation of two simultaneous equations required for the mathematical processing and quantitative analysis of the studied drugs. Alternatively, the partial least squares with and without variable selection procedure (genetic algorithm) have been applied in the spectra analysis because the synchronous inclusion of many unreal wavelengths rather than by using a single or dual wavelength which greatly increases the precision and predictive ability of the methods. Successfully assay of the drugs in their pharmaceutical formulation has been done by the proposed methods. Statistically comparative analysis for the obtained results with the manufacturing methods has been performed. It is noteworthy to mention that there was no significant difference between the proposed methods and the manufacturing one with respect to the validation parameters.
... The aim of the present work was to develop three simple, rapid and selective spectrophotometric methods; namely dual wavelength [21], ratio difference [22] and continuous wavelet transform [22,23] for the determination of MZ in the presence of PYH in pharmaceutical formulations by using less expensive, less toxic and available reagents. On the other hand, PYH can be determined directly at 291 nm where there is no interference from MZ. ...
In this paper, three rapid, simple, accurate and precise spectrophotometric methods were developed for the determination of meclizine hydrochloride in the presence of pyridoxine hydrochloride without previous separation. The methods under study are dual wavelength (DWL), ratio difference (RD) and continuous wavelet transform (CWT). On the other hand, pyridoxine hydrochloride (PYH) was determined directly at 291nm. The methods obey Beer's law in the range of (5-50μg/mL) for both compounds. All the methods were validated according to the ICH guidelines where the accuracy was found to be 98.29, 99.59, 100.42 and 100.62% for DWL, RD, CWT and PYH; respectively. Moreover the precision of the methods were calculated in terms of %RSD and it was found to be 0.545, 0.372, 1.287 and 0.759 for DWL, RD,CWT and PYH; respectively. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of pyridoxine hydrochloride and meclizine hydrochloride in quality-control laboratories.
... This difference is zero for degradate, while it is directly proportional to the concentration of cefadroxil monohydrate. 38,39 In this method, absorbance were measured at λ 1 (230 nm) and λ 2 (265 nm) for both cefadroxil and its degradate. The absorptivity coefficients of each component at both wavelengths were determined by dividing each absorbance over each corresponding concentration. ...
Five simple, accurate, selective and sensitive UV spectrophotometric methods have been developed and validated for the determination of cefadroxil monohydrate in the presence of its alkali-induced degradation product without preliminary separation. These methods include ratio subtraction, absorbance subtraction, amplitude modulation, dual wavelength and simultaneous equation method. These methods were validated and successfully applied for determination of cefadroxil monohydrate in Duricef® capsules. The obtained results were statistically compared with those of the reported method by applying t-test and F-test at 95 % confidence level and no significant difference was observed regarding accuracy and precision.
... These methods include spectrophotometry [2][3][4][5][6][7], spectrofluorimetry [8][9][10], HPLC with UV detection [11][12][13], HPLC with fluorescence detection [14,15], liquid chromatography/mass spectroscopy [16] , capillary elec- trophoresis [17,18] and HPTLC [19]. In the present work a comparative study was done between four methods namely ratio derivative [20], ratio difference [21], mean centering [22] and dual wavelength [23] for the determination of CIP in the presence of its acidic degradation product listing the advantages and the disadvantages of these methods. ...
Four rapid, simple, accurate and precise spectrophotometric methods were used for the determination of ciprofloxacin in the presence of its acidic degradation product. The methods under study are ratio derivative, ratio difference, mean centering and dual wavelength. All the methods were validated according to the ICH guidelines and the obtained accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposedmethodswas tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of ciprofloxacin in quality-control laboratories.
Objective:
The antibiotic metronidazole has been suggested to absorb light at a wavelength range commonly used in spectrophotometric assays. We sought to determine if any of the spectrophotometric assays used in our core laboratory would be susceptible to clinically significant interference from metronidazole in blood-based patient specimens.
Methods:
Following characterization of the absorbance spectrum for metronidazole, spectrophotometric assays involving either main or subtraction wavelengths that might be susceptible to interference from metronidazole were identified. A total of 24 chemistry tests performed on Roche cobas c502 and/or c702 instruments were evaluated for interference from metronidazole. For each assay, two pools of leftover patient serum, plasma, or whole blood specimens containing the analyte of interest at clinically relevant concentrations were prepared. Each pool was spiked with metronidazole at a final concentration of 200 mg/L (1169 µmol/L) or 10 mg/L (58 µmol/L) or the same volume of water as a control, with triplicate samples for each group. The difference in the measured analyte concentration between experimental and control groups was then compared against the total allowable error for each assay to determine whether clinically significant interference had occurred.
Results:
There was no significant interference observed with Roche chemistry tests due to the presence of metronidazole.
Conclusion:
This study provides reassurance that metronidazole is not interfering with the chemistry assays used in our core laboratory. Interference from metronidazole may be a historical problem and current spectrophotometric assays may not be susceptible due to improvements in assay design.
Fourier transform-based algorithms were investigated to resolve UV spectral overlapping of spiramycin and metronidazole in binary mixtures. UV spectra and ratio spectra were both subjected to fast Fourier transform-based first-order differentiation and discrete Fourier transform {i.e. using trigonometric functions such as sin xi – sin (xi + 45⁰), cos xi + cos (xi + 45⁰), sin 2xi – sin 2(xi + 45⁰), cos 2xi + cos 2(xi + 45⁰), sin xi – sin (xi + 60⁰), cos xi + cos (xi + 60⁰)} that followed by 3 passes of 17-point triangular smooth. Such signal transforms generated linear calibration graphs for either drug in the concentration range of 6.25 – 25 mg/L with R² > 0.990. In comparison with the RP-HPLC reference method, the developed UV spectrophotometric methods had no significant difference in terms of accuracy and precision (p > 0.05) when quantifying spiramycin and metronidazole in their coated tablets. They are suggested as analytical quality control methods for their being environmentally friendly, technically simple, quick and economic.
Aspirin and omeprazole combining has proven their effectiveness clinically in the treatment and prevention of cardiovascular diseases in patient with gastric diseases and gastric ulcers. Simultaneous determination of omeprazole and aspirin in their combination is a challenge due to the overlapping spectra of these drugs. Six smart and different spectrophotometric methods were developed for the analysis of omeprazole and aspirin in binary mixture and pharmaceutical dosage form. These smart methods characterized by simplicity and accuracy. The first two methods based on minimal mathematical data processing based on the zero order absorption spectra were; dual wavelength and advanced absorbance subtraction methods. The third method is first and second derivative spectrophotometric method that based on derivative spectra. The last three methods based on ratio spectra manipulation are named; ratio difference, mean centering and derivative ratio spectrophotometric methods. The linearity range of omeprazole was 2-20 μg/mL for dual wavelength method and 2-30 μg/mL for the other ones, while aspirin showed a good linearity over a range of 2.5-30 μg/mL for all methods. The correlation coefficients were greater than 0.999. The results of the developed methods are statistically compared with each other and with the results of the reported HPLC method showing no significant difference. The greenness of the developed methods was assessed using eco-scale scoring method revealing excellent greenness of the applied methods. This spectrophotometric methods is more sensitive and greener with comparing by the reported one so, these developed methods are considered eco-friendly to the environment.
Herein, a simple spectrophotometric method coupled with chemometric techniques i.e. partial least square (PLS) and genetic algorithm (GA) were utilized for the simultaneous determination of the vital ternary antiretroviral therapy dolutegravir (DTG), lamivudine (LMV), and abacavir (ACV) in their combined dosage form. Calibration (25 samples) and validation (13 samples) sets were prepared for these drugs at different concentrations via implementing partial factorial experimental designs. The zero order UV spectra of calibration and validation sets were measured and then subjected for further chemometric analysis. Partial least squares with/without variable selection procedures i.e. genetic algorithm (GA) were utilized to untangle the UV spectral overlapping of these mixtures. Cross-validation and external validation methods were applied to compare the performance of these chemometric techniques in terms of accuracy and predictive abilities. It was found that six latent variables were optimum for modelling DTG, four latent variables for modelling LMV and three latent variables for modelling ACV. Although, good recoveries with prompt predictive ability were attained by these PLS, GA-PLS showed better analytical performance owing to its capability to remove redundant variables i.e. the number of absorbance variables have been reduced to about 21-29 %. The proposed chemometric methods can be reliably applied for simultaneous determination of DTG, LMV, and ACV in their laboratory prepared mixtures and pharmaceutical preparation posing these chemometric methods as worthy and substantial analytical tools in in-process testing and quality control analysis of many antiretroviral pharmaceutical preparations.
For the first time, a fast and simple method was involved to synthesis the flake-like dysprosium molybdate (Dy2MoO6; FL-DyM) nanostructured material on glassy carbon electrode (FL-DyM/GCE) for electrocatalytic analysis of antibiotic drug metronidazole (METZ). The synthesized FL-DyM were systematically characterized by powder X-ray diffraction (XRD), Raman spectroscopy, scanning electron microscopy (SEM), transmission electron microscope (TEM), energy-dispersive X-ray diffraction (EDS), elemental mapping, X-ray photoelectron spectroscopy (XPS), and Brunauer–Emmett–Teller (BET) analysis. The electrochemical properties were scrutinized by cyclic (CV) and differential pulse voltammetry techniques (DPV). The FL-DyM/GCE based sensor demonstrated excellent electrocatalytic activity for METZ detection due to the strong attraction of FL-DyM towards NO2- group in METZ, as well as the more catalytic activity and good electrical conductivity of FL-DyM. The work conditions and finest fabrication were then obtained by thorough optimization of loading suspension, scan rate, and pHs. Compared to the bare GCE and other rare-earth metal molybdates, FL-DyM/GCE sensor showed superior electrocatalytic activity response for METZ detection. The sensor demonstrated a good linear relationship over the concentration range of 0.01-2363 µM. The quantification and detection limits were found to be 0.010 µM and 0.0030 µM, respectively. The FL-DyM/GCE sensor displayed excellent selectivity, repeatability, reproducibility, and stability for detection of METZ in human urine and commercial METZ tablet samples, providing a new technique for efficient drug sensing in practical applications.
Two simple spectrophotometric methods were developed and validated for determination of cefaclor in presence of its acid induced degradation product; namely simultaneous equation method using two wavelengths 265 and 235 nm Method (A) and Area under the curve method using two wavelength ranges (230–240) nm and (260–270) nm Method (B). The accuracy, precision and linearity ranges of the proposed methods were determined. The methods were validated and the specificity was assessed by analyzing synthetic mixtures containing the drug and its degradate. The two methods were applied for the determination of the cited drug in its pharmaceutical preparation and the obtained results were statistically compared with those of a reported method. The comparison showed that there is no significant difference between the proposed methods and the reported method regarding both accuracy and precision.
A simple and effective zeolite modified electrode (ZME) was constructed from Cu(II)-exchanged clinoptilolite nanoparticles (Cu(II)-CNP). The modifier was characterized by FTIR, BET, XRD and TEM techniques. The modified carbon paste electrode (Cu(II)-CNP/CPE) was used for the voltammetric determination of metronidazole (MNZ). The best voltammetric response was obtained by the electrode containing 20% of the modifier in NaCl 0.4 mol L⁻¹ at pH 6. The electrode showed a linear response in the concentration range of 2.0 × 10⁻⁸ to 1.6 × 10⁻⁶ mol L⁻¹ MNZ with a detection limit of 4.1 × 10⁻⁹ mol L⁻¹ from square wave voltammetry. The electrode showed good repeatability, reproducibility, and a long lifetime based on statistical tests. The electrode also has good selectivity and good applicability in the determination of MNZ in some pharmaceutical samples.
A simple, rapid and sensitive isocratic reversed-phase HPLC method with UV detection is described based on external-standard calibration for determination of ciprofloxacin in plasma samples during bioequivalence studies. Both internal and external procedures were evaluated and the external-standard method demonstrated a high validity based on ICH criteria. After protein precipitation with acetonitrile and dichloromethane, chromatographic analysis of ciprofloxacin in plasma was carried out on a μ-bondapack C18 column using acetonitrile:0.005 M tetrabutylammonium bromide (10:90) mixture, pH 2, as mobile phase. Quantitative determination was performed by ultraviolet detector at 278 nm. The method was specific and validated with a limit of detection of 20 ng/ml and limit of quantitation of 50ng/ml. The intra- and inter-day coefficients of variation were in the range of 1.51-4.48% and 4.02-7.3%, respectively. The recovery of method was 94.27±1.91%. The method was applied to a bioequivalence study of two formulations containing 500 mg ciprofloxacin.
In the present paper, two spectrophotometric methods were used for the simultaneous analysis of paracetamol (PCT) and caffeine (CAF) in their laboratory prepared mixtures and pharmaceutical preparations. Simple spectrophotometric analysis of PCT and CAF is not possible due to their complete spectral overlap. The proposed methods are based on the application of continuous wavelet transform (CWT) and derivative transform (using Savitsky–Golay filters) on the ratio spectra to predict each of CAF and PCT. Several wavelet families were tested. Coif1 and Sym2 were found to give best results under optimum conditions. The transformed signals of ratio spectra were used to plot the calibration curves for both components. The predictability of the built calibrations was validated through their application on several synthetic mixtures of both drugs. The proposed methods were used for the prediction of CAF and PCT in pharmaceutical preparation. The obtained results were statistically compared to a reference HPLC method. No significant differences were found between the obtained results and those from the reference method. Being simple, rapid, cheap and sensitive, the proposed methods are recommended for the routine daily analysis of these two drugs in their mixtures in quality control laboratories.
Accurate, selective and sensitive spectrophotometric methods have been developed and validated for simultaneous determination of Cinnarizine and Domperidone, a binary mixture with overlapping spectra, without preliminary separation. These methods include area under the curve (AUC) and dual wavelength spectrophotometry. For the AUC method, the area under curve of mixture solutions in the wavelength ranges 241-258nm and 280-292nm were selected for determination of Cinnarizine and Domperidone and by applying Cramer's rule, concentration of each drug was obtained. In dual wavelength method, two wavelengths were selected for each drug in a way so that the difference in absorbance is zero for another drug. Domperidone shows equal absorbance at 240.2nm and 273.2nm, where the differences in absorbance were measured for the determination of Cinnarizine. Similarly, differences in absorbance at 230.8nm and 259.2nm were measured for determination of Domperidone. The proposed methods were applied for determination of Cinnarizine and Domperidone over the concentration ranges of 2-20 and 2-22μgmL(-1), respectively. The suggested methods were validated as per USP guidelines and the results revealed that they are reliable, reproducible and precise for routine use with short analysis time. The results obtained by the proposed methods were statistically compared to the reported method, and there was no significant difference between them regarding both accuracy and precision.
Two methods are described for the simultaneous determination of ciprofloxacin HCl (CIP) and metronidazole (MET) in binary
mixture. The first method was based on the ion-pair liquid chromatographic separation of the two drugs on reversed-phase,
μBondapak C18 column (250mm×4.6mm, 10μm) Waters. The mobile phase consisted of monobasic potassium phosphate (50mM, pH 3, adjusted
with phosphoric acid) and acetonitrile (65:35, v/v) containing sodium octane sulphonate (50mM). Flow rate of 1.2mLmin−1 was applied. Quantitation was achieved with UV detection at 280nm. Linearity, accuracy and precision were found to be acceptable
over the concentration range of 3–180 and 15–180μgmL−1 for CIP and MET, respectively. The second method was based on the TLC separation of the two drugs followed by densitometric
measurements of their bands at 280nm. The separation was carried out on silica gel 60 F254 plates, using acetonitrile, ammonia, methanol, methylene chloride and hexane (1.3:1.1:2.0:3.0:1.0, v/v) as developing system. The linear regression analysis data were used for the regression line in the range of 1.5–10μg band−1 for CIP and MET. The two proposed methods were successfully applied to the determination of both drugs in laboratory prepared
mixtures and in commercial tablets. The optimized methods proved to be specific, robust and accurate for the quality control
of the cited drugs in pharmaceutical preparation.
KeywordsReversed-phase ion-pair liquid chromatography–TLC densitometry–Antibacterial drugs–Ciprofloxacin hydrochloride–Metronidazole
A binary mixture of ciprofloxacin hydrochloride (CIP) and metronidazole (MET) was determined by five simple and accurate methods, without prior separation. In the first method, CIP was determined by second derivative spectrophotometric method ((2)D) by measuring the amplitude at 282 nm (zero ordinate value of MET). On the other hand, the determination of MET was based on isosbestic point technique, where the total content of the mixture was determined at 294.5 nm (isosbestic point), then the content of MET could be calculated by subtraction. The second method was first derivative ratio spectrophotometric method ((1)DD) where the total amplitude at 261 and 285 nm and the amplitude at 295.5 nm were selected to simultaneously determine CIP and MET in binary mixture, respectively. The third method was based on dual wavelength analysis, in which two wavelengths were selected, at which the absorbances of the other component were the same. The fourth method depends on using Q-analysis method (absorbance ratio) which involves the formation of Q-absorbance equation using the respective absorptivity values at 294.5 nm (isosbestic point) and 281.5 nm (λ(max) of CIP). The fifth method is partial least-squares (PLS) chemometric technique for determination of CIP and MET. The developed methods were successfully applied to the analysis of CIP and MET in laboratory prepared mixtures and tablets with good recoveries and their validation was carried out following the International Conference on Harmonization (ICH) guidelines. The results obtained were statistically compared with each other showing no significant difference with respect to accuracy and precision.
A high-performance thin-layer chromatographic method (HPTLC) has been developed for the determination and the purity control of a synthetic fluoroquinolone antibiotic ciprofloxacin hydrochloride in coated tablets when desfluoro compound, ethylene diamine compound, by-compound A and fluoroquinolonic acid are considered as impurities. Silica gel F254 was used as a stationary phase and a mixture of acetonitrile, ammonia 25%, methanol and methylene chloride (1:2:4:4, v/v/v/v) as a mobile phase. The method was validated in terms of linearity (range), selectivity (placebo and related compounds), precision, accuracy (Recovery), system suitability (repeatability, peak symmetry, resolution) and impurities limit of detection (LOD). The analysis of variance (ANOVA) and t-test were applied to correlate the results of ciprofloxacin hydrochloride determination in coated tablets by means of the HPTLC method and the official British Pharmacopoeia (BP 1999) high-performance liquid chromatographic (HPLC) method.
Capillary zone electrophoresis (CZE) has been elaborated for separation, identification and determination of ciprofloxacin and its impurities. The separation, phosphate buffer pH 6.0 was supplemented with 0.075 M pentane-1-sulfonic acid sodium salt. The elaborated method was validated. The selectivity, linearity, limits of detection (LOD) and quantification (LOQ), precision, and accuracy of capillary zone electrophoresis were evaluated. The results obtained by CZE were also compared with those obtained by liquid chromatography. Regarding the validation results the CE method fulfils the current European Pharmacopoeia (Eur. Ph.) requirements. The evaluated CE method could be applicable to the analysis of different medicinal products containing ciprofloxacin.
A new simple, sensitive and selective liquid chromatography coupled with mass spectrometry (LC-MS) method for quantification of ciprofloxacin in human plasma was validated. Ciprofloxacin and ofloxacin, as internal standard, were analysed on a SB-C18 column (Agilent Technologies, 100 mm × 3 mm I.D., 3.5 μm) under isocratic conditions using a mobile phase of a 70:30 (v/v) mixture of 0.1% (v/v) formic acid in water and acetonitrile. The flow rate was 0.5 mL/min at the column temperature of 25 °C. The detection of the analyte was in SIM mode using a triple quadrupole mass spectrometer with electrospray positive ionisation. The monitored ions were m/z 332 for ciprofloxacin and m/z for 362 for ofloxacin. The sample preparation was very simple and consisted of protein precipitation from 0.2 mL plasma using 0.4 mL of 0.05% acetic acid solution in methanol containing 0.5 mg/mL internal standard. Linear calibration curves were generated over the range of 25-5000 ng/mL with values for coefficient of determination greater than 0.999 and by using a weighted (1/c) linear regression. The lowest limit of quantification was 10 ng/ml. The values of precision (RSD%) and accuracy (relative error%) were less than 8.7% and 11.9%, for within- and between-run, respectively. The recovery of the analyte ranged between 82.5 and 91.1%. Ciprofloxacin demonstrated good stability in various conditions. The validated LC-MS method allows ciprofloxacin monitoring in human plasma during clinical treatment or other pharmacokinetics investigation.
Without resolving mixtures of Cetirizine hydrochloride and Phenylephrine hydrochloride, simultaneous estimation has been successfully achieved by spectrophotometry. First method, simultaneous equation method employs formation and solving of mathematical simultaneous equation using 237.5 nm and 232.0 nm as the λmax of Phenylephrine hydrochloride and Cetirizine hydrochloride respectively in distilled water. Second method is first order derivative spectroscopy, wavelengths selected for quantitation were 232.0 nm for Phenylephrine hydrochloride (zero cross for Cetirizine hydrochloride) and 242.5 nm for Cetirizine hydrochloride (zero cross for Phenylephrine hydrochloride). These methods were validated as per ICH norms. Calibration curves were linear over the concentration ranges of 12-60 μg/ml for both drugs and for both methods. The validation study is statistically significant as all the statistical parameters are within the acceptance range (% RSD < 2.0 and S.D. < 2.0) for both accuracy and precision. The methods are successfully applied to pharmaceutical formulation, with no interference from excipients as indicated by the recovery study. The proposed methods are simple, rapid, economic and accurate for routine simultaneous estimation of Phenylephrine hydrochloride and Cetirizine hydrochloride. Simultaneous equation method was successfully applied to carry out dissolution study of commercial tablet formulation by using USP II dissolution test apparatus.
Two simple, rapid, precise and accurate spectrophotometric methods have been developed for determination of Amlodipine Besylate and Telmisartan by simultaneous equation method and stability study method in combined dosage form. The simultaneous equation method is based on measurement of absorbance at 242 nm and 231 nm as two wavelengths selected for quantification of Amlodipine and Telmisartan. Both methods obeyed Beer's law in the concentration range of 5-30 μg, ml for Amlodipine and 2-7 μg, ml for Telmisartan. Amlodipine and Telmisartan were subjected to stress degradation under different conditions recommended by ICH. The samples so generated were used for degradation studies using the developed method. The proposed methods were validated and can be used for analysis of combined dosage tablet formulation containing Amlodipine and Telmisartan.
Two simple, accurate, precise, sensitive and economic spectrophotometric methods were developed for the simultaneous determination of Simvastatin and Ezetimibe in fixed dose combination products without prior separation. The first method depends on a new chemometrics-assisted ratio spectra derivative method using moving window polynomial least square fitting method (Savitzky-Golay filters). The second method is based on a simple modification for the ratio subtraction method. The suggested methods were validated according to USP guidelines and can be applied for routine quality control testing.
A sensitive, simple and selective high-performance liquid chromatographic (HPLC) method was developed for the determination of ciprofloxacin in biological fluids. The method is based on the reaction between the drug and 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 9.0 to yield a highly fluorescent derivative that is measured at 535 nm after excitation at 464 nm. The calibration curves were linear over the concentration ranges of 25–3000 and 50–3000 ng·mL−1 for plasma and urine, respectively. The mean recovery of ciprofloxacin from plasma and urine was 98.37% and 98.40%, respectively. The method was found to be sensitive, precise, accurate, and reproducible. All of the validation parameters were within the acceptance range.
A facile, ultrasensitive and interference free europium-sensitized spectrofluorimetric method was developed for the simultaneous determination of ciprofloxacin (CFLX), norfloxacin (NFLX), and gatifloxacin (GFLX) in their mixture. A coordination complexes of Eu3+–CFLX/NFLX/GFLX were formed and the coordination was determined using the mole ratio method of continuous variation of equimolar solutions. It was found that the luminescence intensity of Eu3+ for these complexes in their mixtures is quite sensitive to three variant sets of pH, 6.0, 5.5 and 3.5 and excitation wavelengths (λex), 365, 340 and 395 for CFLX, NFLX and GFLX, respectively. Thus a dual-controlled luminescence of smoothly dynamic reversibility is achieved where a reversible on/off switchable emission of one system was observed by tuning its optimal values of pH and λex to the optimal ones of the second and so on for the third. The monitored luminescence intensity of the system showed a good linear relationship with the concentration of CFLX over the range of 5 × 10−8 to 1 × 10−6 mol L−1 with a correlation coefficient of 0.995, for NFLX within a range of 5 × 10−8 to 1.8 × 10−6 mol L−1 with a correlation coefficient of 0.990, and for GFLX within a range of 5 × 10−8 to 1.2 × 10−6 mol L−1 with a correlation coefficient of 0.995. The detection limit (LOD) was determined as 1.5 × 10−8 mol L−1 for CFLX, 3.0 × 10−8 mol L−1 for NFLX and 1.6 × 10−8 mol L−1 for GFLX. The limit of quantification (LOQ) is 4.5 × 10−8, 9.0 × 10−8, 2.8 × 10−8 for CFLX, NFLX and GFLX, respectively. Moreover, a ternary mixture of CFLX, NFLX and GFLX was satisfactorily assessed with average error <4.5%. This method has been successfully validated to the simultaneous and selective determination of CFLX, NFLX and GFLX in pharmaceuticals and serum samples with recoveries of (100.2 ± 2.1, 99.6 ± 2.5 and 103.1 ± 2.9) and (102.9 ± 1.1, 102.5 ± 1.5 and 104.4 ± 3.9), respectively.
An analytical procedure for the determination of ciprofloxacin in serum without previous extraction has been developed. The determination was carried out using iron(III) nitrate as chromogenic agent, with the addition of sodium dodecylsulfate, at pH = 3.0. Absorbance was measured at 430 nm. The range of linearity was between 0.5 – 20.0 μg/mL with a detection limit 0.2 μg/mL.
In order to predict price of candidates in acquisition, in this paper, we design a new model of price prediction of target based on radial basis function neural network. The model is trained by the financial data of acquisition market deals which were made in the past. The result of simulation and test indicates that average error of price prediction is percent 12. It is a suggestive reference of evaluating the feasibility of acquisitions. The result also advises more non-fanance index and training samples should be increased to improve the model.
A simple and inexpensive method for the determination of ciprofloxacin has been developed using solid-phase spectrophotometry. The intrinsic absorbance of ciprofloxacin fixed on a dextran-type cation-exchange resin, Sephadex SP C-25, was measured directly at 277 and 380 nm after packing the gel beads in a 1-mm cell. Using a sample volume of 10 ml, the calibration graph was linear over the range 0.05–0.3 μg ml−1 with a R.S.D. of 1.11% (n=8). The sensitivity obtained is 40 times higher than that of the corresponding solution method. The method was applied to the determination of ciprofloxacin in pharmaceutical preparations and was validated by standard addition.
Ciprofloxacin was given orally to 28 healthy male volunteers for single oral dose of 500mg; Plasma samples were collected at different time's interval between 0 and 12h and analyzed both by high pressure liquid chromatography and by a microbiological assay. The detection limits (LOD) were 0.02μg/ml and 0.1μg/ml, for both methods respectively. For each method, coefficients of variation (R(2)) were 0.9995 and 0.9918 in plasma and limit of quantitation (LOQ).02 and 0.5μg/ml. The Comparison of means maximum concentration 2.68 μg/ml at 1.5 hr for test and 2.43 μg/ml are attain in HPLC method of Reference at 2hrs respectively. The plasma concentrations measured by microbiological assay of reference tablet are 3.95μg/ml (mean ± SE) at 1 hour and 3.80μg/ml (mean ± SE) at 1 hour. The concentrations in plasma measured by microbiological method were markedly higher than the high-pressure liquid chromatography values which indicates the presence of antimicrobially active metabolites. The mean ± SE values of pharmacokinetic parameters calculated by HPLC method, for total area under the curve (AUC 0-oo) were 13.11, and 11.91 h.mg/l for both test and reference tablets respectively. The mean ± SE values of clearance measured in l/h were 44.91 and 48.42 respectively. The elimination rate constant Kel [l/h] showed 0.17 l/h for test and 0.15 l/h reference tablets and likewise, absorption half-life expressed in hours shown 0.67 h for test and 1.04 h for reference respectively. The Mean Residence Time for test is 5.48 h and 5.49 h for reference. The mean ± SE values of pharmacokinetic parameters (Microbiological assay) for total area under the curve (AUC 0-oo) were 22.11 and 19.33 h.mg/l for both test and reference tablets respectively. The mean ± SE values of clearance measured in l/h were 29.02 and 31.63 respectively. The elimination rate constant Kel [l/h] showed 0.21 l/h for test and 0.20 l/h reference tablets and likewise, absorption half-life expressed in hours shown 0.86h for test and 0.56 h for reference respectively. The Mean Residence Time for test is 5.27 h and 4.67 h for reference. Significant difference observed between two methods.
Sequential Signals in ChemistryBasicsLinear FiltersCorrelograms and Time Series AnalysisFourier Transform TechniquesTopical Methods
Problems
A method for the determination of trace amounts of ciprofloxacin has been developed, based on solid-phase spectrofluorimetry. The relative fluorescence intensity of ciprofloxacin fixed on Sephadex SP C-25 gel was measured directly after packing the gel beads in a 1-mm silica cell, using a solid-phase attachment. The wavelengths of excitation and emission were 272 and 448 nm, respectively. Using a sample volume of 1000 ml, the linear concentration range of application was 0.3-10.0 ng.ml(-1) of ciprofloxacin, with a R.S.D. of 1.2% (for a level of 4.0 ng.ml(-1)) and a detection limit of 0.1 ng.ml(-1). The method was applied to the determination of ciprofloxacin in human urine and serum samples. It was validated applying the standard addition methodology and using HPLC as a reference method. Recovery levels of the method reached 100% in all cases.
Ciprofloxacin has a reduced activity against anaerobic pathogens. Therefore, a combination of ciprofloxacin with an antimicrobial agent active against anaerobes, such as metronidazole, seems to be interesting for the treatment of mixed aerobic/anaerobic infections. High metronidazole concentrations (10 mg/l or 40 mg/l) neither affected the bactericidal efficacy of ciprofloxacin on aerobic pathogens, such as Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa and Enterococcus faecalis, nor on the anaerobic pathogens Clostridium perfringens and Clostridium difficile, as demonstrated by kill-kinetic curves. The same high concentrations, as well as lower therapeutically achievable concentration (2 mg/l or 5 mg/l) of metronidazole in combination with ciprofloxacin were slightly more potent for the tested clostridia than ciprofloxacin or metronidazole alone.
A method to determine plasma concentrations of ciprofloxacin and its metabolite desethyleneciprofloxacin (M1) by CE with HeCd laser-induced fluorescence detection is described. Following precipitation of proteins and centrifugation supernatant is injected hydrodynamically (10 s, 0.5 p.s.i.) into the capillary. Overall analysis time for the quantification of both analytes was 7 min. The total amount of plasma needed for multiple injections (n>5) was 10-20 microl. Data on accuracy and precision are presented. The assay performance is compared to the specifications of a validated HPLC method, which is routinely used for the quantification of ciprofloxacin and M1 in body fluids. Both methods showed comparable accuracy and precision for both analytes throughout the whole working range (inter-day precision <9%; inter-day accuracy 96-110%). The limit of quantification (LOQ) of 20 microg/l (M1 10 microg/l) for the CE procedure was slightly higher than for the HPLC method, where 10 microg/l (M1 2.5 microg/l) was determined. However, application of the methods to human plasma samples derived from a clinical study proved that comparable results are obtained and that the sensitivity of the HPCE method was sufficient to fully describe typical plasma concentration time profiles of ciprofloxacin and its metabolite M1. Both the adequate sensitivity and the required smaller sample volume compared to HPLC indicate that the method is feasible for clinical studies where sample amounts are limited, e.g., studies to investigate pharmacokinetics in pediatric patients. Preclinical studies form another possible application of this technique.
A spectrophotometric method was described for the determination of the antibacterial quinolone derivatives, ciprofloxacin, enrofloxacin and pefloxacin through charge transfer complex formation with three different acceptors. Chloranilic acid (CL) was utilized for their determination, forming charge transfer complex with lambdamax 520 nm. The proposed method was applied for determination of Ciprocin tablets, Enroxil oral solution, Peflacin ampoules and Peflacin tablets, with mean percentage accuracies, 99.58+/-1.25,99.94+/-0.96,100.91+/-1.59 and 99.86+/-1.003. Also, tetracyanoethylene (TCNE) was utilized in the determination of the concerned compounds forming charge transfer complexes with maximum absorbances at lambdamax 335 nm for ciprofloxacin and at lambdamax 290 nm for both enrofloxacin and pefloxacin. The procedure was applied for determination of Ciprocin tablets, Enroxil 10% oral solution, Peflacine tablets and Peflacine ampoules with mean percentage accuracies 99.40+/-1.27,99.95+/-0.90,98.98+/-1.565 and 99.88+/-0.998, respectively. Also, 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) was utilized for determination of pefloxacin forming charge transfer complex with maximum absorbance at lambdamax 460 nm. The procedure was applied for determination of peflacine tablets and peflacine ampoules with mean percentage accuracies 100.40+/-0.76 and 99.91+/-0.623, respectively. Statistical analysis of the obtained results showed no significant difference between the proposed method and other official and reported methods as evident from the t-test and variance ratio.
A simple flow injection UV spectrophotometric sensing device was developed for the determination of ciprofloxacin. The method is based on its transient retention and concentration on Sephadex SP C-25 cation-exchange gel beads packed in the flow cell and the continuous monitoring of its native absorbance on the solid phase at 277 nm. The procedure is carried out without any derivatisation. Formic acid/NaOH 1.75 M at pH 2.2 is used as carrier solution in a simple monochannel FIA manifold. When the analytical signal reached the maximum value, ciprofloxacin was eluted from the solid support by the carrier solution itself. The response of the sensor was linear in the concentration range 0.5-10 microg ml(-1) with an RSD (%) of 0.79, a detection limit (3sigma criterion) of 0.035microg ml(-1) and a sampling rate of 16 h(-1). Application to the analysis of pharmaceutical samples testifies the utility of this sensor.
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